CN105776873B - A kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization - Google Patents
A kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization Download PDFInfo
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- CN105776873B CN105776873B CN201610323135.0A CN201610323135A CN105776873B CN 105776873 B CN105776873 B CN 105776873B CN 201610323135 A CN201610323135 A CN 201610323135A CN 105776873 B CN105776873 B CN 105776873B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002425 crystallisation Methods 0.000 title claims abstract description 23
- 230000008025 crystallization Effects 0.000 title claims abstract description 22
- 238000001816 cooling Methods 0.000 title claims abstract description 21
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 16
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000004080 punching Methods 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 239000013081 microcrystal Substances 0.000 claims abstract description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract 3
- 230000008018 melting Effects 0.000 claims abstract 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 28
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- 239000011787 zinc oxide Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 239000006004 Quartz sand Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 5
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims 2
- 238000004321 preservation Methods 0.000 claims 1
- 238000009738 saturating Methods 0.000 claims 1
- 230000009466 transformation Effects 0.000 claims 1
- 235000019801 trisodium phosphate Nutrition 0.000 claims 1
- 239000000156 glass melt Substances 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000010583 slow cooling Methods 0.000 abstract description 4
- 230000009477 glass transition Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000003303 reheating Methods 0.000 abstract 1
- 230000002269 spontaneous effect Effects 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 238000000048 melt cooling Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000004031 devitrification Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000146 host glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000006132 parent glass Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- -1 phosphoric acid hydrogen Chemical class 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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Abstract
The present invention relates to glass field of new materials, the high-crystallinity transparent glass-ceramics of more particularly to a kind of " melting cooling " method crystallization.With SiO2、Al2O3、P2O5、Na2O、K2O, MgO, ZnO are made of effective material according to certain weight proportion.Preparation method includes raw material mixing and uniform batch is made, by batch after 1480 ~ 1510 DEG C of meltings keep the temperature 3 hours, the glass melt of homogenizing is cast in the punching block of 880 DEG C ~ 950 DEG C preheatings, Glass Transition is then down to 15 ~ 25 DEG C/min of cooling velocity in fine annealing stove（T g）Temperature, cooled to the furnace after annealed 30 minutes ~ 1 hour room temperature high-crystallinity transparent microcrystal glass material.The present invention makes its sufficient crystallising in slow cooling procedure, and then obtain high-crystallinity, eliminates secondary reheating process of traditional high-crystallinity transparent glass-ceramics in preparation method by controlling the cooling velocity in crystallization temperature section.
Description
Technical field
The present invention relates to a kind of sides that high-crystallinity transparent glass-ceramics is prepared using crystallization spontaneous in melt cooling process
Method belongs to glass field of new materials.
Background technology
Transparent glass-ceramics is widely used to building decoration, laser gain medium and display because of its good physicochemical property
Field, physicochemical property and the crystalline content in devitrified glass are closely related, therefore usually require that and obtain high crystallinity as possible.
About high-crystallinity, it will be appreciated that the volume content for crystal in devitrified glass is higher（Generally higher than 50%）；On the other hand it is appreciated that
For for certain given crystal form, practical crystallinity/theory crystallinity is close to 1.0.In general, people are using at parent glass heat
Logos obtains high-crystallinity, i.e., the glass melt of homogenizing first is obtained parent phase glass by various forming methods, then pass through again
Heat treatment makes parent phase devitrification of glass.It is well known that thermodynamically the energy of devitrified glass is low compared with its parent phase glass, glass melt
In cooling procedure there are the trend of spontaneous crystallization, if it is brilliant to be precipitated glass melt under the premise of product molding is not influenced
Body does not need to then be heat-treated parent glass, greatlys save the energy, has good economic and social benefit.Milkiness glass
Glass is exactly to be prepared using this feature（Referring to patent：Borrelli N F. Fast response photosensitive
opal glasses. U.S. Patent 4,979,975, (1990)）, that is, refraction is precipitated in glass melt in cooling procedure
Rate differs larger crystal of fluoride with host glass, and then leads to its milkiness.The patent of invention of the present inventor is a kind of using molten
Body cools down the transparent glass-ceramics of spontaneous crystallization（Application number：201110003480.3）Once report utilized " melting-cooling " legal system
Standby transparent glass-ceramics, but the preparation condition of patent of invention report is to be quickly cooled down process, since melt viscosity is cooled
It is increased rapidly in journey so that crystallizing insufficient, therefore crystallinity is not high.
For the crystallized glass article of crystallization spontaneous in this kind of melt cooling process, high-crystallinity should be obtained again
High transparency is kept, it is necessary to meet following condition：Crystallization mode is body crystallization rather than Surface Crystallization first, this requires glass to form
Nucleation curve and crystal growth curve have it is largely be overlapped；Secondly the refractive index of crystal and the refractive index of host glass
It approaches, to prevent devitrification caused by scattering strongly；Again, it for given crystal type, is tied to practical crystallinity/theory
For brilliant degree close to 1.0, the cooling velocity of glass melt should not be too fast, especially should not mistake in the increase of crystallization range viscosity
Soon.Up to the present, it yet there are no and prepare high-crystallinity using crystallization spontaneous in glass melt cooling procedure（Practical crystallinity/reason
By crystallinity close to 1.0）The report of transparent glass-ceramics.
Invention content
In order to make up for the deficiencies of the prior art, the present invention provides the high knots that a kind of preparation method is simple, raw material are easy to get
Brilliant degree（I.e.：Practical crystallinity/theory crystallinity>90%）Transparent glass-ceramics.
The present invention is achieved through the following technical solutions：
A kind of high-crystallinity transparent glass-ceramics of spontaneous crystallization, it is characterized in that, by effective material of following weight fraction
It is made：SiO2：（55.55~58.35%）, Al2O3：（0~6.23%）, P2O5：（8.46~8.89%）, Na2O：（9.24~19.41%）,
K2O：（0~14.05%）, MgO：（4.21~4.42%）, ZnO：（8.50~8.93%）.
The present invention obtains high-crystallinity transparent glass-ceramics using spontaneous crystallization during glass melt Slow cooling process.
In glass melt cooling procedure, it is 10 to measure viscosity by rotary process3.0Still without there is crystallization during Pa S, glass disclosure satisfy that
The various molding needs of glass product.
The present invention makes it that Na be precipitated during Slow cooling by adjusting the composition of glass melt3PO4Or AlPO4It is brilliant
Body, and its practical crystallinity/theory crystallinity is more than 90%.The devitrified glass is not needed to crystallized glass article after molding
The step of being heat-treated again, can be with the effectively save energy.
The present invention more excellent scheme be：
The fusion temperature of the material prescription is 1480 ~ 1510 DEG C, and melt is cast in 880 DEG C ~ 950 after keeping the temperature 3 hours
DEG C preheating punching block in, Glass Transition is then down to 15 ~ 25 DEG C/min of cooling velocity in fine annealing stove（Tg）Temperature
Degree, room temperature is cooled to the furnace after annealed 30 minutes ~ 1 hour.
Effective material SiO2Source for quartz sand, Al2O3Source for aluminium hydroxide, P2O5Source be phosphoric acid hydrogen
Diammonium, Na2The source of O be sodium carbonate, K2The source of O is potassium carbonate, and the source of MgO is magnesia, and the source of ZnO is zinc oxide.
Compared with prior art, the method for the high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization of the invention
Possessed advantageous effect is：Glass melt by the way of slow cooling, makes it in crystallization range after cast molding
Interior viscosity is pushed the speed relatively slowly, and then is conducive to the precipitation of crystal, and it is required in traditional high-crystallinity devitrified glass production to overcome
Heat treatment process, not only technical process is simple, easily operated, and can the effectively save energy, reduce production cost.Separately
Outside, the refractive index of glass parent phase and crystal is very close to advantageously reducing light scattering, it ensure that crystallite dimension is more than 300nm
In the case of still keep the high grade of transparency, be a kind of high-crystallinity transparent glass-ceramics new material with wide application prospect.
Description of the drawings
Fig. 1 is the X-ray powder diffraction pattern of high-crystallinity transparent glass-ceramics in embodiment 1；
Fig. 2 is the optical transmission spectra figure of high-crystallinity transparent glass-ceramics in embodiment 1.
Specific embodiment
Below by way of specific embodiment to a kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization of the invention
It is described further.
Embodiment 1：
Raw materials used parts by weight form：58.64 parts of quartz sand（It is equivalent to 58.35 parts of SiO2）, diammonium hydrogen phosphate
16.80 parts（It is equivalent to 8.89 parts of P2O5）, 33.88 parts of sodium carbonate（It is equivalent to 19.41 parts of Na2O）, 4.51 parts of magnesia（It is equivalent to
4.42 part MgO）, 9.02 parts of zinc oxide（It is equivalent to 8.93 parts of ZnO）.
3 hours are kept the temperature in 1480 DEG C of electric furnace after being weighed, be mixed evenly by above-mentioned composition, the glass melt of homogenizing is poured
In the punching block for casting from 930 DEG C of preheatings, then dropped from 930 DEG C to 520 with 15 DEG C/min of cooling velocity in fine annealing stove
DEG C, cooled to the furnace after annealed 30 minutes room temperature blocky water white transparency microcrystal glass material；Its thickness be 3.0mm when
Transmitance at 650nm wavelength is 90%, and the crystal of precipitation is Na3PO4, crystallinity 95%.
Embodiment 2：
Raw materials used parts by weight form：55.83 parts of quartz sand（It is equivalent to 55.55 parts of SiO2）, diammonium hydrogen phosphate
15.99 parts（It is equivalent to 8.46 parts of P2O5）, 16.13 parts of sodium carbonate（It is equivalent to 9.24 parts of Na2O）, 20.97 parts of potassium carbonate（It is equivalent to
14.05 part K2O）, 4.29 parts of magnesia（It is equivalent to 4.21 parts of MgO）, 8.58 parts of zinc oxide（It is equivalent to 8.50 parts of ZnO）.
Weighed by said components, be mixed evenly after keep the temperature 3 hours in 1490 DEG C of electric furnace, the glass melt of homogenizing is poured
In the punching block for casting from 880 DEG C of preheatings, then 520 are down to from 880 DEG C in fine annealing stove with 15 DEG C/min of cooling velocity
DEG C, cooled to the furnace after annealed 30 minutes room temperature blocky water white transparency microcrystal glass material；Its thickness be 3.0mm when
Transmitance at 650nm wavelength is 92%, and the crystal of precipitation is Na3PO4, crystallinity 91%.
Embodiment 3：
Raw materials used parts by weight form：57.20 parts of quartz sand（It is equivalent to 56.91 parts of SiO2）, diammonium hydrogen phosphate
16.39 parts（It is equivalent to 8.67 parts of P2O5）, 24.78 parts of sodium carbonate（It is equivalent to 14.20 parts of Na2O）, 10.74 parts of potassium carbonate（Quite
In 7.2 parts of K2O）, 4.40 parts of magnesia（It is equivalent to 4.31 parts of MgO）, 8.79 parts of zinc oxide（It is equivalent to 8.70 parts of ZnO）.
Weighed by said components, be mixed evenly after keep the temperature 3 hours in 1500 DEG C of electric furnace, the glass melt of homogenizing is poured
In the punching block for casting from 880 DEG C of preheatings, then 520 are down to from 880 DEG C in fine annealing stove with 15 DEG C/min of cooling velocity
DEG C, cooled to the furnace after annealed 30 minutes room temperature blocky water white transparency microcrystal glass material；Its thickness be 3.0mm when
Transmitance at 650nm wavelength is 92%, and the crystal of precipitation is Na3PO4, crystallinity 94%.
Embodiment 4：
Raw materials used parts by weight form：57.21 parts of quartz sand（It is equivalent to 56.92 parts of SiO2）, aluminium hydroxide 9.63
Part（It is equivalent to 6.23 parts of Al2O3）, 16.39 parts of diammonium hydrogen phosphate（It is equivalent to 8.67 parts of P2O5）, 26.44 parts of sodium carbonate（It is equivalent to
15.15 part Na2O）, 4.40 parts of magnesia（It is equivalent to 4.31 parts of MgO）, 8.80 parts of zinc oxide（It is equivalent to 8.71 parts of ZnO）.
It weighs, be mixed evenly by said components, then keep the temperature 3 hours in 1510 DEG C of electric furnace, the glass of homogenizing is melted
Body is poured in the punching block for casting from 950 DEG C of preheatings, is then down in fine annealing stove with 25 DEG C/min of cooling velocity from 950 DEG C
Cooled to the furnace after 560 DEG C, annealed 1 hour room temperature blocky water white transparency microcrystal glass material；When its thickness is 3.0mm
Transmitance at 650nm wavelength is 93%, and the crystal of precipitation is AlPO4, crystallinity 96%.
The above described is only a preferred embodiment of the present invention, be not that the invention has other forms of limitations, it is ripe
The equivalent reality of equivalent variations can be made modifications based on the technical contents disclosed above or be modified as by knowing those skilled in the art
Apply example.It is all without departing from technical solution of the present invention content, technical spirit according to the present invention makees above example any
Simple modification, equivalent variations and remodeling still fall within the protection domain of technical solution of the present invention.
Claims (3)
1. a kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization, it is characterized in that, by having for following weight fraction
Effect material is made：SiO2 55.55~58.35%、Al2O3 0~6.23%、P2O5 8.46~8.89%、Na2O 9.24~19.41%、K2O
0~14.05%、MgO 4.21~4.42%、ZnO 8.50~8.93%；The material mixed melting temperature is 1480 ~ 1510 DEG C, heat preservation
Melt is cast in the punching block of 880 DEG C ~ 950 DEG C preheatings after 3 hours, then with 15 ~ 25 DEG C/min in fine annealing stove
Cooling velocity be down to glass transformation temperature, cool to room temperature with the furnace after annealed 30 minutes ~ 1 hour, it is saturating to obtain high-crystallinity
Bright devitrified glass.
2. the high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization according to claim 1, it is characterised in that：
The principal crystalline phase of the transparent microcrystal glass material is Na3PO4 or AlPO4 crystal, after crystallisation by cooling at a slow speed its practical crystallinity/
Theoretical crystallinity is more than 90%.
3. the high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization according to claim 1, it is characterised in that：
The source of effective material SiO2 is quartz sand, and the source of Al2O3 is aluminium hydroxide, and the source of P2O5 is diammonium hydrogen phosphate,
The source of Na2O is sodium carbonate, and the source of K2O is potassium carbonate, and the source of MgO is magnesia, and the source of ZnO is zinc oxide.
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| CN201610323135.0A CN105776873B (en) | 2016-05-17 | 2016-05-17 | A kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization |
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| CN201610323135.0A CN105776873B (en) | 2016-05-17 | 2016-05-17 | A kind of high-crystallinity transparent glass-ceramics of " melting-cooling " method crystallization |
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| CN108623154B (en) * | 2018-07-10 | 2021-04-23 | 齐鲁工业大学 | Surface-strengthened transparent glass |
| CN108821570B (en) * | 2018-07-10 | 2021-06-08 | 山东康友光电科技股份有限公司 | Formula and method for preparing surface-strengthened transparent plate glass |
| CN113200678B (en) * | 2021-03-18 | 2022-06-10 | 常熟佳合显示科技有限公司 | Glass material, preparation method thereof and product thereof |
| CN115286251B (en) * | 2022-08-10 | 2024-02-23 | 清远南玻节能新材料有限公司 | Tempered glass, microcrystalline glass and preparation method and application thereof |
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| CN102173589B (en) * | 2011-01-10 | 2013-01-09 | 山东轻工业学院 | Transparent microcrystalline glass by spontaneous devitrification during fusant cooling |
| CN103073190B (en) * | 2013-02-21 | 2014-12-24 | 山东轻工业学院 | Spontaneously-crystallized up-converting luminescent transparent ceramic glass |
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